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All 7 posts Subject: Amt-nitrostyrene? Please login to post Down

Grignard
(Hive Bee)
11-09-04 23:15
No 540714
      Amt-nitrostyrene?

I condensated indole-3-carboxaldehyde with nitroethane as in the ultrasound promoted nitrostyrene dokument at rodiums page.. i tested the reaction mix on tlc after 3 h but i got a lot of aldehyde left and let the mix stand over night.. when i came next morning there was a lot of small yellow crystalls in the bottom of the round bottom and the aldehyde was almost gone (by tlc), so i evaporated the solvent and try to rextallize from boiling MeOH.. but the yellow crystaline mass do not solved. And when i put it in the fridge a lot of needle like brown crystalls start to form.. what could this yellow crystalls be and is the styrene from this compound brown needels? should i filter the yellow mass from the hot MeOH and proceed to the next step with the brown crystalls? diffused?? yes... tongue tongue

hest
(Hive Adickt)
11-10-04 07:57
No 540781
      Xtals

Overnight with UltraSound ???
The typical polutant is the dimer, and that's a dead end.
disolve the material in app 10mL MeOH/g decant the MeOH from the brown stuff and put the MeOH in the fridge.

Ant next tim follow your reation home, dont let them sit.

Grignard
(Hive Bee)
11-10-04 08:11
No 540783
      so the ultrasound has destroyed some of the...

so the ultrasound has destroyed some of the material? But this synt vasn`t any good for this aldehyde, because the aldehyde remains unsolved in the nitroethane throgh the sonication.. aldehyde was purchased from a lab company.. So all the yelow stuff must be filtered from the meOH and i will proceed with the crystalls that solved in hot MeOH.. I followed the procedure just as it stands on rhodium..

hest
(Hive Adickt)
11-11-04 08:49
No 540992
      Aldehyde

1: test on TLC, are there more aldehyde ???
2: you will have two yellow spot's, one is the TM the other is the polymer

and yess, evaporate the nitroethane (or frezz and filter) and then eksrakt then seperate the polymer from the TM. You might have to rextalise the material after the seperation.
Alternative bee a pig, frezz the nitroethane and material, filter off all the material, reduce the chunk with LAH and the clean the amine.

Grignard
(Hive Bee)
11-11-04 15:53
No 541031
      Yes, there was more aldehyde after 20 h with...

Yes, there was more aldehyde after 20 h with sonication!!? i checked and double checked the procedure to se if i have forgotten any thing, but it seems alright.. I got to yellow spot on tlc as you say, and a wery fluorising blue spot with rf = 0 on 50 % EtOAc in hexane. and a wery weak spot from the aldehyde. This aldehyde is not wery soluble so next time i will try to add another solvent beside the Nitroethane. This procedure is great for trimethoxy-aldehyde by the way.... wink Thanks for your reply hest.. i now got some brownish/yellow needles that is the righ styrene. The polymer was filtered from the hot MeOH and then soluted in acetone and crystallised just to see what this stuff is..

starlight
(Hive Bee)
11-11-04 19:27
No 541063
      indole carboxaldehyde

I found indole-3-carboxyaldehyde condensations with 1-nitropropane to be a real bitch. Loads of aldehyde left over, or loads of polymerized crap, or both. And low yields.

It will be much easier with nitroethane. If you are having problems, then you could try the procedure here as it it works better than any other for the nitropropane condensation:

Post 514779 (starlight: "Satisfactory condensation method", Tryptamine Chemistry)

But you will probably need to run the condensation for only 3 hours rather than 7 if you are using nitroethane. The 55C refers to the bath temperature not the reaction temp. Still if you are doing TLC you will be able to get it just right.

Grignard
(Hive Bee)
11-12-04 12:20
No 541218
      thanks.. i know the methylamine condensation...

thanks.. i know the methylamine condensation is good, but it is so much work to make.. he he.. lazy boy.. I got a lot of paraformaldehyde here but i will have to make hexamethylenetetramine. I havent measured the yield from this above synth yet, but i will report it over the weekend.

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	All 7 posts		Subject: Amt-nitrostyrene?		Please login to post		Down


		Grignard (Hive Bee) 11-09-04 23:15 No 540714				Amt-nitrostyrene?
						I condensated indole-3-carboxaldehyde with nitroethane as in the ultrasound promoted nitrostyrene dokument at rodiums page.. i tested the reaction mix on tlc after 3 h but i got a lot of aldehyde left and let the mix stand over night.. when i came next morning there was a lot of small yellow crystalls in the bottom of the round bottom and the aldehyde was almost gone (by tlc), so i evaporated the solvent and try to rextallize from boiling MeOH.. but the yellow crystaline mass do not solved. And when i put it in the fridge a lot of needle like brown crystalls start to form.. what could this yellow crystalls be and is the styrene from this compound brown needels? should i filter the yellow mass from the hot MeOH and proceed to the next step with the brown crystalls? diffused?? yes...



		hest (Hive Adickt) 11-10-04 07:57 No 540781				Xtals
						Overnight with UltraSound ??? The typical polutant is the dimer, and that's a dead end. disolve the material in app 10mL MeOH/g decant the MeOH from the brown stuff and put the MeOH in the fridge. Ant next tim follow your reation home, dont let them sit.



		Grignard (Hive Bee) 11-10-04 08:11 No 540783				so the ultrasound has destroyed some of the...
						so the ultrasound has destroyed some of the material? But this synt vasn`t any good for this aldehyde, because the aldehyde remains unsolved in the nitroethane throgh the sonication.. aldehyde was purchased from a lab company.. So all the yelow stuff must be filtered from the meOH and i will proceed with the crystalls that solved in hot MeOH.. I followed the procedure just as it stands on rhodium..



		hest (Hive Adickt) 11-11-04 08:49 No 540992				Aldehyde
						1: test on TLC, are there more aldehyde ??? 2: you will have two yellow spot's, one is the TM the other is the polymer and yess, evaporate the nitroethane (or frezz and filter) and then eksrakt then seperate the polymer from the TM. You might have to rextalise the material after the seperation. Alternative bee a pig, frezz the nitroethane and material, filter off all the material, reduce the chunk with LAH and the clean the amine.



		Grignard (Hive Bee) 11-11-04 15:53 No 541031				Yes, there was more aldehyde after 20 h with...
						Yes, there was more aldehyde after 20 h with sonication!!? i checked and double checked the procedure to se if i have forgotten any thing, but it seems alright.. I got to yellow spot on tlc as you say, and a wery fluorising blue spot with rf = 0 on 50 % EtOAc in hexane. and a wery weak spot from the aldehyde. This aldehyde is not wery soluble so next time i will try to add another solvent beside the Nitroethane. This procedure is great for trimethoxy-aldehyde by the way.... Thanks for your reply hest.. i now got some brownish/yellow needles that is the righ styrene. The polymer was filtered from the hot MeOH and then soluted in acetone and crystallised just to see what this stuff is..



		starlight (Hive Bee) 11-11-04 19:27 No 541063				indole carboxaldehyde
						I found indole-3-carboxyaldehyde condensations with 1-nitropropane to be a real bitch. Loads of aldehyde left over, or loads of polymerized crap, or both. And low yields. It will be much easier with nitroethane. If you are having problems, then you could try the procedure here as it it works better than any other for the nitropropane condensation: Post 514779 (starlight: "Satisfactory condensation method", Tryptamine Chemistry) But you will probably need to run the condensation for only 3 hours rather than 7 if you are using nitroethane. The 55C refers to the bath temperature not the reaction temp. Still if you are doing TLC you will be able to get it just right.



		Grignard (Hive Bee) 11-12-04 12:20 No 541218				thanks.. i know the methylamine condensation...
						thanks.. i know the methylamine condensation is good, but it is so much work to make.. he he.. lazy boy.. I got a lot of paraformaldehyde here but i will have to make hexamethylenetetramine. I havent measured the yield from this above synth yet, but i will report it over the weekend.

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